CN105085224B - A kind of method that hypericin is extracted from hypericum perforatum - Google Patents
A kind of method that hypericin is extracted from hypericum perforatum Download PDFInfo
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- CN105085224B CN105085224B CN201510541490.0A CN201510541490A CN105085224B CN 105085224 B CN105085224 B CN 105085224B CN 201510541490 A CN201510541490 A CN 201510541490A CN 105085224 B CN105085224 B CN 105085224B
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- C07C46/00—Preparation of quinones
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Abstract
The invention discloses a kind of method that hypericin is extracted from hypericum perforatum, comprise the steps:Immersion treatment, Feedstock treating, digest, deoil, alkali carries, column chromatography, drying.The present invention first extracts vegetable fat using enzyme, separated using non-oil component to oily different with the affinity difference and profit proportion of water by oily with non-oil component, add product yield and improve recovery rate, the hypericin that the present invention is obtained, content is more than 0.5% (UV detections), and ash content is below 7%.
Description
Technical field
The present invention relates to the extracting method of biological technical field, specifically one kind extracts hypericin from hypericum perforatum
Method.
Background technology
Hypericum perforatum (Hypericum perforatum L) also known as Herba Hyperici Monogyni, St. john's wort (St.John's
Wont), it is Guttiferae hypericum, is distributed widely in Europe, Asia, African the north, Australia, South and North America, is for people
One of herbal medicine that class more early recognizes and utilized, has point on China Henan, Hebei, Shandong, Shaanxi, Gansu, Sichuan, Xinjiang and other places
Cloth.Hypericum perforatum is under the jurisdiction of Guttiferae, Hypericum.Perennial herb, it is high 20-60 centimetres, it is all hairless.Stem is in cylinder,
Long l0-100cm, multi-branched, stem and branch both sides respectively have a vertical rib, and sprig is carefully thin, to being born in axil.Single leaf is to life, stockless
Stem, blade lanceolar or oblong are embraced, long 1-2cm, wide 0.3-0.7cm spread transparent or black gland point, and black gland point is big
It is distributed in blade edge or nearly top more.Cyme basidixed, flower yellow, each 5 of calyx, petal, Long Circle or lanceolar, side
Edge has black gland point；Stamen is most, and symphysis is 3 beams, style 3.Gas is micro-, and mildly bitter flavor is puckery.The month at florescence 6-7, the fruiting period 8-9 months.Property is pungent,
It is cold.
Hypericum perforatum is as Chinese traditional herbs, and herb contains hypericin, with the content highest of petal, with it is clearing heat and detoxicating,
The effects such as anti-inflammation, promotion wound healing.With going deep into for modern pharmacology activity research, it is in antiviral, antidepression, anti-swollen
Effect in terms of knurl is increasingly paid close attention to by the mankind.Hypericum perforatum is embodied in pharmacopeia by countries such as Germany, the U.S..
Hypericin (Hypericin) is the most material of bioactivity in hypericum perforatum, with convergence, antibacterial, only
The effect such as blood, clearing and activating the channels and collaterals and antiviral and antitumor, antidepression and photo-activity.Hypericin is carried by the herb of hypericum perforatum
Take and obtain, Main Ingredients and Appearance is extract of hypericum perforatum, hypericin, gas delicate fragrance, bitter is soluble in water.With depression,
Antiviral effect.Also can be as veterinary drug, for chicken group's preventing and treating bird flu.
The existing technique applied in production is as solvent, sodium hydroxide balancing alkalinity acidity, the life of this technique with methanol
The product yield of output is low, and Determination of Hypericin from Extraction is in 0.28-0.33%, and ash content severe overweight.Now with the expansion in market
And competition, the need for 0.3% hypericin can not meet international customers, American-European client needs 0.4% and more than 0.4%
Hypericin, ash requirements are below 8%, and traditional technique can not directly produce the hypericin of 0.4% content.
The content of the invention
It is simple with technique it is an object of the invention to provide a kind of method that hypericin is extracted from hypericum perforatum, fit
Symphysis is produced, the low advantage of production cost.
The present invention is achieved through the following technical solutions, a kind of method that hypericin is extracted from hypericum perforatum, specific bag
Include following steps：
1) immersion treatment：Hypericum perforatum is loaded into woven bag, mouth is tied, is placed in pond, pond topped up with water, and in pond
Weight in upper face pressure, immersion；
2) Feedstock treating：By step 1) obtained hypericum perforatum crushes, adds pure equivalent to 2-3 times of weight of raw material
Water, is heated to 50-60 DEG C of maintenance 5-10min, obtains paste serous material；
3) digest：By step 2) obtained paste serous material, tune pH is 4-5, adds paste serous material 0.05-0.1% parts by weight
Pectin-cellulose complex enzyme and 0.001 parts by weight mannitol carry out enzymolysis 40-60min, obtain enzymolysis liquid；
4) deoil：By step 3) obtained enzymolysis liquid, the pure water of 2-3 times of weight is added, 60-70 DEG C of extraction is heated to
60-120min, obtains upper strata oil slick liquid and subnatant, slag mixture, separation；
5) alkali carries：To step 4) obtained subnatant, slag mixture add alkali lye, extracted；
6) column chromatography：Combining step 5) extract solution is obtained, acid adding adjusts pH to 3-4, and centrifugation obtains supernatant, concentrates, use macropore
Polymeric adsorbent is adsorbed, and resin is cleaned with deionized water to trickle to be colourless, then with concentration is 75-80% (v/v)
Ethanol solution is eluted, and collects eluent；
7) dry：Eluent is concentrated, medicinal extract is obtained, then by being dried to obtain hypericin.
Step 1 of the present invention) described in immersion, time preferred 15-24h.
Step 3) described in pectin-cellulose complex enzyme, preferably activity be the active units of 1-3 ten thousand/gram solid-state pectin-fibre
Tie up complex enzyme.
Step 5) described in alkali carries, be preferably added to 0.1M NaOH solution, addition is step 4) obtained subnatant, slag
3-5 times of volume of mixture, heating extraction 2 times, 80-100 DEG C of temperature, each 30-60min.
Step 6) described in centrifugation, preferably rotating speed be 3500r/min, time 10min, described macroreticular resin
It is preferred that D101 types, HPD100 types.
Compared with prior art, advantages of the present invention：
1st, contain grease in the plant cell of hypericum perforatum, mainly by composition for triglycerides compound group into mixing
Thing, these greases irregularly divide with elaioleucite and oil body protoplast form, in discontinuous graininess, together with granule protein body
Existence form is present in disseminated cell etc..Existing extracting method, is all after directly the raw materials such as hypericum perforatum are smashed or crushed
Directly extracted by modes such as water extraction/alcohol extracting or Microwave Extractions, when extracting, the grease in cell can be separated simultaneously
Go out, group and hypericin (Hypericin), pseudohypericin (Pseudohypericin) containing grease, former hypericin
(Protohypericin), former hypericin (Protopseudohypericin), ring pseudohypericin
(Cyclopseudoyhypericin), different hypericin (Isohypericin), rheum emodin-anthrone (Emodin-
Anthrone), the composition such as pigment mixes, so as to influence the separation of follow-up active ingredient, adds the intractability of process.
The present invention first using enzyme extract vegetable fat, using non-oil component to oil it is different with the affinity difference and profit proportion of water and incite somebody to action
It is oily to be separated with non-oil component, add product yield and improve recovery rate.
2nd, the present invention is using the immersion of hypericum perforatum pond, and hypericum perforatum is immersed in water, gradually softened, and moisture enters naturally
To inside, beneficial to the separation of vegetable fat, beneficial to subsequently digesting, deoil；Meanwhile, it is immersed in water, anaerobic bacteria amount reproduction,
Particularly summer when, can souring, pH value can reduce, the adjustment pH of convenient process below.
3rd, the present invention first removes the grease in cell membrane, release plant cell using pectin-cellulose complex enzyme, adds sweet
Reveal alcohol, osmotic pressure can be kept, beneficial to the release of grease, while pigment can also be destroyed, obtained product color is than existing production
Product are shallow.
4th, the hypericin that the present invention is obtained, content is more than 0.5% (UV detections), and ash content is below 7%.
Embodiment
With embodiment, the invention will be further described below, but the invention is not limited in these embodiments.
Embodiment 1：
A kind of method that hypericin is extracted from hypericum perforatum, specifically includes following steps：
1) immersion treatment：Hypericum perforatum is loaded into woven bag, mouth is tied, is placed in pond, pond topped up with water, and in pond
Weight in upper face pressure, soaks 24h；
2) Feedstock treating：By step 1) obtained hypericum perforatum crushes, and adds the pure water equivalent to 2 times of weight of raw material,
60 DEG C of maintenance 5min are heated to, paste serous material is obtained；
3) digest：By step 2) obtained paste serous material, it is 5 to adjust pH, adds the activity of the parts by weight of paste serous material 0.05%
Be 30,000 active units/gram solid-state pectin-fiber composite enzyme and 0.001 parts by weight mannitol carry out enzymolysis 40min, obtain
Enzymolysis liquid；
4) deoil：By step 3) obtained enzymolysis liquid, the pure water of 2 times of weight is added, 60 DEG C of extraction 120min are heated to,
Obtain upper strata oil slick liquid and subnatant, slag mixture, separation；
5) alkali carries：To step 4) obtained subnatant, slag mixture add 3 times of volume 0.1M NaOH solution, and heating is carried
Take 2 times, 100 DEG C of temperature, each 60min；
6) column chromatography：Combining step 5) extract solution is obtained, acid adding adjusts pH to 3, centrifuges, 3500r/min, 10min obtain supernatant
Liquid, concentration, is adsorbed with D101 type macroporous absorbent resins, and it is colourless that resin to trickle is cleaned with deionized water, then is used
Concentration elutes for 75% ethanol solution, collects eluent；
7) dry：Eluent is concentrated, medicinal extract is obtained, then by being dried to obtain hypericin, detected through UV, content
0.52% (UV detections), ash content 6.5%.
Embodiment 2：
A kind of method that hypericin is extracted from hypericum perforatum, specifically includes following steps：
1) immersion treatment：Hypericum perforatum is loaded into woven bag, mouth is tied, is placed in pond, pond topped up with water, and in pond
Weight in upper face pressure, soaks 18h；
2) Feedstock treating：By step 1) obtained hypericum perforatum crushes, and adds the pure water equivalent to 3 times of weight of raw material,
50 DEG C of maintenance 8min are heated to, paste serous material is obtained；
3) digest：By step 2) obtained paste serous material, it is 4.5 to adjust pH, adds the activity of the parts by weight of paste serous material 0.1%
Be 20,000 active units/gram solid-state pectin-fiber composite enzyme and 0.001 parts by weight mannitol carry out enzymolysis 50min, obtain
Enzymolysis liquid；
4) deoil：By step 3) obtained enzymolysis liquid, the pure water of 3 times of weight is added, 65 DEG C of extraction 90min are heated to,
Obtain upper strata oil slick liquid and subnatant, slag mixture, separation；
5) alkali carries：To step 4) obtained subnatant, slag mixture add 4 times of volume 0.1M NaOH solution, and heating is carried
Take 2 times, 90 DEG C of temperature, each 30min；
6) column chromatography：Combining step 5) extract solution is obtained, acid adding adjusts pH to 4, centrifuges, 3500r/min, 10min obtain supernatant
Liquid, concentration, is adsorbed with HPD100 type macroporous absorbent resins, and it is colourless that resin to trickle is cleaned with deionized water, then
Eluted with concentration for 80% ethanol solution, collect eluent；
7) dry：Eluent is concentrated, medicinal extract is obtained, then by being dried to obtain hypericin, detected through UV, content
0.55% (UV detections), ash content 6.7%.
Embodiment 3：
1) immersion treatment：Hypericum perforatum is loaded into woven bag, mouth is tied, is placed in pond, pond topped up with water, and in pond
Weight in upper face pressure, soaks 15h；
2) Feedstock treating：By step 1) obtained hypericum perforatum crushes, and adds the pure water equivalent to 2 times of weight of raw material,
55 DEG C of maintenance 10min are heated to, paste serous material is obtained；
3) digest：By step 2) obtained paste serous material, it is 4 to adjust pH, adds the activity of the parts by weight of paste serous material 0.05%
Be 10,000 active units/gram solid-state pectin-fiber composite enzyme and 0.001 parts by weight mannitol carry out enzymolysis 60min, obtain
Enzymolysis liquid；
4) deoil：By step 3) obtained enzymolysis liquid, the pure water of 2 times of weight is added, 70 DEG C of extraction 60min are heated to,
Obtain upper strata oil slick liquid and subnatant, slag mixture, separation；
5) alkali carries：To step 4) obtained subnatant, slag mixture add 5 times of volume 0.1M NaOH solution, and heating is carried
Take 2 times, 80 DEG C of temperature, each 45min；
6) column chromatography：Combining step 5) extract solution is obtained, acid adding adjusts pH to 3, centrifuges, 3500r/min, 10min obtain supernatant
Liquid, concentration, is adsorbed with DHPD100 type macroporous absorbent resins, and it is colourless that resin to trickle is cleaned with deionized water, then
Eluted with concentration for 75% ethanol solution, collect eluent；
7) dry：Eluent is concentrated, medicinal extract is obtained, then by being dried to obtain hypericin, detected through UV, content
0.53% (UV detections), ash content 6.8%.
Claims (5)
1. a kind of method that hypericin is extracted from hypericum perforatum, it is characterised in that comprise the following steps：
1) immersion treatment：Hypericum perforatum is loaded into woven bag, mouth is tied, is placed in pond, pond topped up with water, and on pond
Weight in pressure, immersion；
2) Feedstock treating：By step 1) obtained hypericum perforatum crushes, and adds the pure water equivalent to 2-3 times of weight of raw material, plus
Heat obtains paste serous material to 50-60 DEG C of maintenance 5-10min；
3) digest：By step 2) obtained paste serous material, tune pH is 4-5, adds the fruit of paste serous material 0.05-0.1% parts by weight
Glue-cellulose complex enzyme and the mannitol of 0.001 parts by weight carry out enzymolysis 40-60min, obtain enzymolysis liquid；
4) deoil：By step 3) obtained enzymolysis liquid, the pure water of 2-3 times of weight is added, 60-70 DEG C of extraction 60- is heated to
120min, obtains upper strata oil slick liquid and subnatant, slag mixture, separation；
5) alkali carries：To step 4) obtained subnatant, slag mixture add alkali lye, extracted；
6) column chromatography：Combining step 5) extract solution is obtained, acid adding adjusts pH to 3-4, and centrifugation obtains supernatant, concentrates, use macroporous absorption
Resin is adsorbed, and resin is cleaned with deionized water to trickle to be colourless, then the ethanol solution for being 75-80% with concentration is washed
It is de-, collect eluent；
7) dry：Eluent is concentrated, medicinal extract is obtained, then by being dried to obtain hypericin.
2. a kind of method that hypericin is extracted from hypericum perforatum according to claim 1, it is characterised in that：Step 1)
Described immersion, the time is 15-24h.
3. a kind of method that hypericin is extracted from hypericum perforatum according to claim 1, it is characterised in that：Step 3)
Described pectin-cellulose complex enzyme, be activity be the active units of 1-3 ten thousand/gram solid-state pectin-fiber composite enzyme.
4. a kind of method that hypericin is extracted from hypericum perforatum according to claim 1, it is characterised in that：Step 5)
Described alkali carries, refer to the NaOH solution for adding 0.1M, and addition is step 4) obtained subnatant, the 3- of slag volume of mixture
5 times, heating extraction 2 times, 80-100 DEG C of temperature, each 30-60min.
5. a kind of method that hypericin is extracted from hypericum perforatum according to claim 1, it is characterised in that：Step 6)
Described macroreticular resin is D101 types, HPD100 types.
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| CN201510541490.0A CN105085224B (en) | 2015-08-31 | 2015-08-31 | A kind of method that hypericin is extracted from hypericum perforatum |
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| CN106668088A (en) * | 2017-02-08 | 2017-05-17 | 内蒙古昶辉生物科技股份有限公司 | Preparation method of hyperforin perforatum extract |
| CN109394843B (en) * | 2019-01-03 | 2021-03-26 | 重庆工商大学 | Method for preparing hypericum perforatum extract rich in hypericin |
| CN115872848B (en) * | 2022-12-27 | 2024-03-26 | 陕西嘉禾药业有限公司 | Method for preparing hypericin qualified by polycyclic aromatic hydrocarbon by using Hypericum perforatum |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1436562A (en) * | 2002-02-08 | 2003-08-20 | 湖北丽益医药科技有限公司 | Hypericum perforatum extract and its prepn process and medicine composition |
| CN101759549A (en) * | 2009-11-20 | 2010-06-30 | 南京泽朗医药科技有限公司 | Method for preparing hypericins |
| CN101829164A (en) * | 2010-05-07 | 2010-09-15 | 河南中医学院 | Biological preparation method of Hypericum perforatum L extractive |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1436562A (en) * | 2002-02-08 | 2003-08-20 | 湖北丽益医药科技有限公司 | Hypericum perforatum extract and its prepn process and medicine composition |
| CN101759549A (en) * | 2009-11-20 | 2010-06-30 | 南京泽朗医药科技有限公司 | Method for preparing hypericins |
| CN101829164A (en) * | 2010-05-07 | 2010-09-15 | 河南中医学院 | Biological preparation method of Hypericum perforatum L extractive |
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